Two-step synthesis of triarylmetals (As, Sb, Bi) starting from the metal oxides and 2,6-dimethoxybenzenethiol

Article abstract of DOI:10.1016/S0022-328X(97)00421-X

Reported here is a new synthetic method of triarylmetals MAr₃ (M = As, Sb, Bi). It is composed of two-step reactions starting from the metal oxides: (1) A reaction of the metal oxide with 2,6-dimethoxybenzenethiol ΦSH [Φ = 2,6-(MeO)₂C₆H₃] in the presence of acid to give the thiolatometals M(SΦ)₃, and (2) A reaction of M(SΦ)₃ with organolithium reagent LiAr to give MAr₃ (Ar = Ph, 4-MeC₆H₄, 4-Me₂NC₆H₄, Φ). Since ΦSH is odorless and crystalline, most of it can be recovered after the reactions without difficulty for repeated usages. The intermediates M(SΦ)₃ are also crystalline and inert against hydrolysis.